Method of determining the grease content of fibers



March 5, 1940. MACKENZlE 2,192,614

- METHOD OF DETERMINING THE GREASE CONTENT OF FIBERS Filed Jan. 29, 1938 2 Sheets-Sheet 1 INVENT OR.

VMwo

ATTORNEYJ.

F. H. MACKENZIE 2,192,614

METHOD OF DETERMINING THE GREASE CONTENT OF FIBERS Filed Jan. 29, 1938 I I Y i j ;i% C i m. 1 v z 5/ I 5 E IL 7? 1 7 INVENTOR.

M w. W Y

ATTORNEYJ.

2 Sheets-fSheet 2- 5 volatile solvent.

Patented Mar. 5, 1940 NlTED STATES METHOD OF-DETERMINING THE GREASE CONTENT OF FIBERS Franklin HQ Macken'zie, Bywood, Pa., assignor to American Chemical Paint Company, Ambler,

'Pa., a corporation of Delaware Application January 29, 1938, Serial No. 181,579

2 Claims.

This invention relates to a method and apparatus for measuring. The-invention is particularly concerned with the determination of the content of non-volatile matter dissolved in a Still more specifically, the invention is especially suitable in determining the content of wax, grease, oil, etc. in textile fibers,

or in liquors containing such substances removed from the fibers (either. in suspension, emulsion 10 or solution), such as liquors which'have been used to scour, cleanse, or degrease the fibrous materials. v

While the invention is described and claimed hereinafter with particular reference to the dee termination of the grease content in .textile fibers, it is to be understood that the invention j is capable of a variety of adaptations for analogous uses. It is further noted that in carrying out the invention as applied to the determination ofthe grease content in wool or the like, the measurement, broadly speaking, is accomplished by'solution of the grease in a volatile solvent, evaporation of the solvent, and weighing of the residual grease.

Before considering many of the objects and advantages of the invention, thefollowing comments are presented in connection with the technical .problems encountered in this field.

, In the conduct of cleaning operations on fibrous materials, it is frequently necessary to be sure that a definite quantity of soluble material be left in the cleaned product. For example, in

. wool scouring, the operation must be carried out in a manner to ensure the presence of a definite residual grease content. Too little residual grease results in a harsh wool and in high fiber breakage, as well as noils" in the combing op- .q eration. Too high a content of residualgrease causes other technical diflieulties', or indicates an imperfectly scoured wool. a

Another consideration of substantial importance is that for many purposes it is desirable to obtain a determination of grease content in wool in a very short time, in order that the operator of a scouring process may be advised soon enough for him toappropriately adjust the of the general type here under consideration have frequently beencarried out byja continuous extraction apparatus such, f or instance, as the Soxhlet apparatus. In following this practice it is usual to subject a weighed sample of the j material, such as wool fibers/to the action of'a volatile solvent in which the extractable sub-. stances but not the fibers are soluble,.until all the 'soluble material hasbeen extracted. .The solvent is then evaporated from the'extract'by heating in a beaker or other suitable vessel on a steam or water bath, until all butthe last traces.

. as splashing, bumping gor creeping of,the .material over the edge of the vessel during evaporation, with the result that some materialis lost andthe determination or. calculation made correspondingly inaccurate; While initial hea t' ing of the evaporating vessel by means of a steam or water bathis of some aid in overcoming splashing and fbumping, these expedients do not affect ,creeping. I,

, With the foregoing in mind, the primary object of the present "invention isthe provision of a method and apparatus for, the general purpose'shere involved, in accordance with; which ,determinationS may be made withinan ex- ,10 of the solvent are removed. Thereafter the last 1 tremely short period of time. By way of example, inathedetermination of the grease content in wool, my-invention provides for the obtaining of a result in as littleas ten minutes.

' Inaddition to the foregoing, the invention contemplates overcoming many of the technical difficulties heretofore encountered, such as splashing, bumping and creeping,

Still 'furthen'in' accordance with the invention, equipment is provided of a-c'onvenient and readily portable nature, the equipment incorporating' the essentialdevices employedin mak-' ing determinations of this kind and preferably being operable by meansof the commonly available sources of electric current, so that the unit .may be fplugged inat virtuallyany convenient location.

of the present invention is carried'out as follows; A predetermined volume of an appropriate sol- "Very generallyand briefly stated, the method 7 20, dition, technical difficulties are encountered such vent is poured over a suitable weighed sample of fibrous material. A mortar is desirably employed for this purpose and a plunger is used to macerate the fibers in the presence of the solvent in the mortar. A convenient aliquot part of the solvent is then poured ofi or expressed from the fibers and the solvent thus removed contains an aliquot part of the total soluble matter in or on the fibers.

This sample of a grease laden solvent is then treated to evaporate the solvent in accordance with the method and apparatus described more fully hereinafter, which provides for very rapid evaporation without loss from creeping or other causes.

With the foregoing in mind, reference is now made to the drawings illustrating the preferred embodiment of the apparatus and in which:

Figure 1 is a sectional elevational view of the equipment with certain of the parts appearing in elevation and the major portion of the casing structure shown in section substantially on the line l--l of Figure 2, with the lower left hand portion thereof taken substantially on the line la,la of Figure 2;

Figure 2 is a top view of Figure 1 with the cover and certain parts of the equipment removed;

Figure 3 is a vertical section taken substantially on the line 3-3 of Figure 1 with certain parts of the equipment-removed;

' Figure 4 is a view in side elevation oi the evaporating vessel;

Figure 5 illustrates a suitable mortar and plunger for use in preparing a sample for treatment; and

Figure 6 is a view illustrating a measuring device preferably employed. a

The casing 1 is generally of squared box shape having convenient supporting pads or the like 8. Within the casing a motor 9 is carried as by angle brackets ill, with one end of the motor projecting through the casing wall as at H. A double wire electric cord 2| is provided for connection of the motor to any convenient source of current, a switch 22 being interposed in the circuit for control purposes. A fan or blower I2 is associated with the other end of the motor, this fan delivering air to the conduit l3.

which extends downwardly and forwardly (to the left when viewed as in Figure 1) and in the discharge end M the conduit is provided with an electrical heating element I5. Air is supplied to the fan 12 centrally through an opening in the end wall l6 of the casing therefor. Air may be drawn into the motor and fan chamber through apertures I! provided in the outer end ll of the motor which projects externally of the casing, for motor cooling purposes, and also through apertures 18, here shown as conveniently located in the bottom wall of the'casing.

Partitions 19 form an evaporating chamber into which the discharge end 14 of the blower mechanism projects. Access to the evaporating chamber is had by means of a displaceable cover plate 20 positioned on the front wall of the unit as clearly seen in Figures 1 and 2. Upon removal or displacement of this cover, the evaporating vessel C (shown in detail in Figure 4) may be inserted into the evaporating chamber.

The motor chamber is closed at the top by means of the wall 23, this wall having three pockets or wells 24,25 and 26 recessed therein for the purpose of receiving and carrying separately handleable units described hereinafter,

which are used in association with the apparatus. A hinge mounted cover 21 having a closure catch 2329 is provided in order to completely enclose the devices carried in the wells 24, 25 and 26. The cover is equipped with a handle providing for ready portability of the entire equipment.

Turning now to Figure 5, the mortar is indicated at 3| and the plunger at 32, this plunger having a head 33 of such size as to fit somewhat loosely within the inside of the mortar and thus permit effecting a squeegee action upon placing measured quantities of wool fibers and solvent in the mortar.

The measuring -vessel 34 shown in Figure 6 is made of transparent material and provided with graduations 35 and 36, the latter representing an aliquot part of the former. The purpose of this measuring device and the manner of its graduation will be apparent from the following description of the entire determination process and manipulation of the apparatus.

A predetermined measured quantity (for ex-- ample 5 grams) of wool fibers is first placed in the mortar 3| and then solvent is measured in the device 34 to the upper graduation 35 (representing, for example, 29 ml.) and this quantity added to the wool fibers in the mortar 3|. For convenience, a supply or bottle of solvents (such as carbon tetrachloride) is kept in the pocket forced thoroughly through the wool. The mortar is then allowed to stand for a few minutes (about two) with the plunger on top of the wool, after which the solvent is again forced through the wool by pumping an additional number of times (suitably about twenty-five).

Grease-containing solvent is now measured in the device 34 up to the graduation 36 (representing for purposes of illustration 13 ml.). It will be found that the wool must usually be squeezed slightly to obtain this exact amount.

This measured quantity of grease-containing solvent is then poured into the cup C shown in Figure 4, the capacity of this cup preferably being such as to provide a liquid level therein at about the point indicated at L, and in any event at some point well below the upper lip or edge of the cup. The cup is then placed in the evaporating chamber, after displacement of the closure 20 and the switch 22 is thrown on in order to start the motor and heat the element [5. It may here be noted that during the evaporating operation the cover 0 for the cup is not employed, it being desirable that the heated air delivered from the discharge end l4 of the blower come in contact with and pass over the a surface of the liquid in the cup.

The proportioning oi the batch of material (13 ml. in the example given above) and the total volumetric capacity of the evaporating cup in a manner to provide a relatively low liquid level therein is of importance in providing against loss, especially by creeping. This end is also served by making the cup of some material (for example aluminum or copper) of relatively high heat conductivity. With these two provisions, the result of the blowing of the heated air into the cup and around the side walls thereof is to maintain a relatively high temperature in the side walls of the cup above the liquid level of the sample being determined. This relatively high temperature in turn results in extremely rapid before it reaches the upper edge or passes over the edge. This avoids losses which have introduced errors in calculations of this type heretofore in consequenceoi'handling of the cup or cleaning or wiping the outside surface. thereof prior toweighing,

At the same time, the air directly on to the surface of the liquid in the cup carries away the evaporated. -solvent ata high rate and this, in turn, promotes further evaporation, as a result of which evaporation is carried on very rapidly.

After complete evaporation (usually accomplished in about three minutes), the lid c is replaced on the cup and it is allowed to cool to room temperature and then re-weighed. The desired calculations are then made to determine the content ofgrease in the sample tested.

In connection with the foregoing, it should be understood that in many respects the-description of the proportions and the like is given merely by way of example and not as limiting the scope of the invention;

In addition,'the method and apparatus may be employed for purposes other than determining the grease content in wool, as has already been stated. For instance, the invention may be employed to determine the content of a suspended fat in an emulsion. This .may be eflected by placing a measured amount of the emulsion in a separator-y funnel and agitating with a quantity of water-immiscible solvent placed in the measuring vessel 34 up to the graduation 35.

,Aiter the separation of the solvent layer, suflicient of that layer is measured into the device 34 to fill it up to the graduation 36, and this portion thereafter placed in the evaporating cup C and the process carried out. as already described above.

It will also be obvious that numerous detailed changes may be made in theshape, size, proportionaand dispositions of parts or the apparatus,

45 without departing item the spirit of the invenblowing of the heated tion. By wayof illustration, if desired, the air circulation apertures and passages may be quite differently arranged and the air and evaporated solvent passing out of the opening in the evaporating chamber may be carried away by a suitable conduit for discharge either'to an exhaust hood or to some point exterior of the building in which the tests are made.

, In accordance with the foregoing, the invention accomplishesa number of improvements in this art and notably the invention provides forthe making of determinations very quickly and without errors which have heretofore been unavoidable,.,at"le ajst in equipment of a commercial type providing for reasonably rapid determinations.

' I claim:

. 1. In the art of deternnning' the grease of wool fibers, the method which includes madn ating a batch of wool fibers in. the presence of a grease solvent, placing an aliquot batch ,of the grease laden solvent in an evaporating vessel of capacity substantially greater than the batch to leave the upper edges of the side walls of the vessel exposed, effecting evaporation of the solvent and maintaining a higher temperature in the wall of the vessel above the level of said batch than below said level by directing a stream of 'heated air over'the exposed surfaces of the vessel and over the surface of the liquid therein, and

measuring the residual grease.

2. In the art of determining the grease content of wool fibers, the method which includes macer- 'ating a batch of wool fibers in the presence of a grease solvent, placing an aliquot batch of the grease laden solvent in an evaporating vessel of capacity substantially greater than the batch to leave the upper edges'of the side walls of the vessel exposed, efiecting evaporation of the solvent by application of heat in a manner to maintain higher temperature injthe side walls of the vessel above the surface'level of liquid therein as compared with the temperature below said level, and measuring the residual grease.

mm n. mcxauzm. 

